Reaktion #433679

Reaktionsgleichung

acetic acid

(6-chloropyridazin-3-yl)hydrazine

triethylamine

3-cyanobenzoyl chloride

water

→

3-(6-chloro-1,2,4-triazolo[4,3-b]pyridazin-3-yl)benzonitrile

Lösungsmittel

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwith cooling in ice
2. 2
   Filtrationthe precipitate was collected by filtration
3. 3
   Waschenwashed with water and diethyl ether
4. 4
   Sonstigeto obtain
5. 5
   workup.STIRRINGthe mixture was stirred at 110° C. for 2 hours
6. 6
   Einengenthe reaction solution was concentrated under reduced pressure
7. 7
   Waschenthe resultant crude crystal was washed with ethanol

Vorschrift

To a solution of (6-chloropyridazin-3-yl)hydrazine and triethylamine in THF, 3-cyanobenzoyl chloride was added with cooling in ice, and stirred at room temperature for 1 hour. The reaction solution was combined with water, and the precipitate was collected by filtration, washed with water and diethyl ether to obtain, N′-(6-chloropyridazin-3-yl) -3-cytanobenzohydrazide. To this, acetic acid was added, and the mixture was stirred at 110° C. for 2 hours, the reaction solution was concentrated under reduced pressure, and the resultant crude crystal was washed with ethanol to obtain 3-(6-chloro-1,2,4-triazolo[4,3-b]pyridazin-3-yl)benzonitrile. Dat (F:256).

Quelle